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Eingeladener Vortrag
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Accurate and reproducible measurement of the structure and properties of high-value nanoparticles is extremely important for their commercialization. A significant proportion of engineered nanoparticle systems consist of some form of nominally core-shell structure, whether by design or unintentionally. Often, these do not form an ideal core-shell structure, with typical deviations including polydispersity of the core or shell, uneven or incomplete shells, noncentral cores, and others. Such systems may be created with or without intent, and in either case an understanding of the conditions for formation of such particles is desirable. Precise determination of the structure, composition, size, and shell thickness of such particles can prove challenging without the use of a suitable range of characterization techniques. Here, the authors present two such polymer core-shell nanoparticle systems, consisting of polytetrafluoroethylene cores coated with a range of thicknesses of either polymethylmethacrylate or polystyrene. By consideration of surface energy, it is shown that these particles are expected to possess distinctly differing coating structures, with the polystyrene coating being incomplete. A comprehensive characterization of these systems is demonstrated, using a selection of complementary techniques including scanning electron microscopy, scanning transmission electron microscopy, thermogravimetric analysis, dynamic light scattering, differential centrifugal sedimentation, and X-ray photoelectron spectroscopy. By combining the results provided by these techniques, it is possible to achieve superior characterization and understanding of the particle structure than could be obtained by considering results separately.
To properly understand and assess the long-term behaviour of geosynthetic materials it is necessary to investigate the various types of possible degradation mechanims. This includes both chemical and mechanical behaviour, and sometimes even their interactions with one another. Clearly, chemical degradation of geosynthetics depends on the polymer type. For example, polyolefins are vulnerable to oxidation; polyesters are susceptible to hydrolysis; and plasticizers can leach from polyvinyl chloride. This paper describes the concept of these three types of degradation, but focuses on the oxidation of polyolefins since the majority of the geosynthetics is made from this type of polymer. The methods used to predict the lifetime of antioxidants and service life of the geosynthetic material will be illustrated. Furthermore, the influence of temperature, pressure, and ultraviolet light on the service life are also demonstrated. Finally, the current specifications targeting the longevity of different geosynthetics are presented.
Regarding mechanical degradation, the paper mainly focuses upon the creep deformation of geogrids and stress crack resistance (SCR) of polyethylene geomembranes and geopipe. The method to assess stress crack resistance is described, and the microscopic mechanisms that lead to such failure are explained. For creep evaluation, different acceleration tests are presented and their applicability with respect to the different types of polymers is illustrated. In addition, the long-term shear behaviour of geocomposites and geosynthetic clay liners is presented.
Zur Sicherung von Deponien und Altlasten mit dem Ziel eines langfristig wirksamen Grundwasserschutzes werden seit Mitte der 80er Jahre Kombinationsdichtungen (Verbund aus Kunststoffdichtungsbahn und mineralischen Dichtschichten) eingesetzt. Um deren Langzeitbeständigkeit auch unter extremen Bedingungen bewerten zu können, wurden Permeationsmesszellen, welche die Verhältnisse in der Deponie nachstellen und über einen Zeitraum von 12 Jahren mit einem Mehrkomponentengemisch konzentrierter organischer Verbindungen beaufschlagt worden waren, zerlegt und die Auswirkungen der Schadstoffpermeation auf die Abdichtungsmaterialien untersucht. Schwerpunkte der hier vorgestellten Arbeiten waren Untersuchungen: - zur Auswirkung der Permeation des Gemisches an organischen Verbindungen auf die Eigenschaften der Kunststoffdichtungsbahn, - zur vertikalen Verteilung der organischen Verbindungen in den mineralischen Dichtungen, - zu Veränderungen mineralogischer, mikromorphologischer und bodenmechanischer Eigenschaften der mineralischen Dichtungsmaterialien, - zu mikrobiellen Aktivitäten in den mineralischen Dichtungen. Daneben wurden Stofftransportparameter bestimmt und eine Modellierung des Stofftransportes durchgeführt. Die verschiedenen untersuchten Materialien der Kombinationsdichtungen erwiesen sich unter den extremen Bedingungen als ein stabiles und effizientes Abdichtungssystem.
Long term behaviour of composite liners under exposure to a mixture of concentrated hydrocarbons
(1999)
Composite liners (a geomembrane in intimate contact with a mineral liner) are frequently used to line landfills and contaminated sites. It is therefore very important to characterise the behaviour of these systems even under extreme conditions.
An investigation was undertaken to determine the influence of a mixture of concentrated organic contaminants on composite liner materials taken from test cells that had been dismantled after a 12-year permeation test.
The organic hydrocarbons had permeated the HDPE-geomembrane and had then migrated or had been adsorbed within the mineral liners, depending on their properties. The obtained concentration profiles of the contaminant mixture components indicate that the various mineral layer materials have selective retardation abilities which correspond to the different parameters of the organic compounds as well as of the mineral layer.
In addition, contaminant transport in the composite liners tested was modelled and the results of the model analysis compared with measurement data. An example (acetone) illustrates the calculated spatial and temporal contaminant concentration.
The composite liners investigated exhibit a very good sealing capacity against the concentrated organic contaminants used.
This is a corrigendum to the original article "Determining the thickness and completeness of the shell of polymer core-shell nanoparticles by X-ray photoelectron spectroscopy, secondary ion mass spectrometry, and transmission scanning electron microscopy" that was published in "The journal of physical chemistry C", vol. 123 (2019), no. 49 pp. 29765-29775.
Core–shell nanoparticles (CSNPs) have become indispensable in various industrial applications. However, their real internal structure usually deviates from an ideal core–shell structure. To control how the particles perform with regard to their specific applications, characterization techniques are required that can distinguish an ideal from a nonideal morphology. In this work, we investigated poly(tetrafluoroethylene)–poly(methyl methacrylate) (PTFE–PMMA) and poly(tetrafluoroethylene)–polystyrene (PTFE–PS) polymer CSNPs with a constant core diameter (45 nm) but varying shell thicknesses (4–50 nm). As confirmed by transmission scanning electron microscopy (T-SEM), the shell completely covers the core for the PTFE–PMMA nanoparticles, while the encapsulation of the core by the shell material is incomplete for the PTFE–PS nanoparticles. X-ray photoelectron spectroscopy (XPS) was applied to determine the shell thickness of the nanoparticles. The software SESSA v2.0 was used to analyze the intensities of the elastic peaks, and the QUASES software package was employed to evaluate the shape of the inelastic background in the XPS survey spectra. For the first time, nanoparticle shell thicknesses are presented, which are exclusively based on the analysis of the XPS inelastic background. Furthermore, principal component analysis (PCA)-assisted time-of-flight secondary-ion mass spectrometry (ToF-SIMS) of the PTFE–PS nanoparticle sample set revealed a systematic variation among the samples and, thus, confirmed the incomplete encapsulation of the core by the shell material. As opposed to that, no variation is observed in the PCA score plots of the PTFE–PMMA nanoparticle sample set. Consequently, the complete coverage of the core by the shell material is proved by ToF-SIMS with a certainty that cannot be achieved by XPS and T-SEM.
The fluorolytic sol–gel synthesis is applied with the intention to obtain two different types of core–shell nanoparticles, namely, SrF2–CaF2 and CaF2–SrF2. In two separate fluorination steps for core and shell formation, the corresponding metal lactates are reacted with anhydrous HF in ethylene glycol. Scanning transmission electron microscopy (STEM) and dynamic light scattering (DLS) confirm the formation of particles with mean dimensions between 6.4 and 11.5 nm. The overall chemical composition of the particles during the different reaction steps is monitored by quantitative Al Kα excitation X-ray photoelectron spectroscopy (XPS). Here, the formation of stoichiometric metal fluorides (MF2) is confirmed, both for the core and the final core–shell particles. Furthermore, an in-depth analysis by synchrotron radiation XPS (SR-XPS) with tunable excitation energy is performed to confirm the core–Shell character of the nanoparticles. Additionally, Ca2p/Sr3d XPS intensity ratio in-Depth profiles are simulated using the software Simulation of Electron Spectra for Surface Analysis (SESSA). In principle, core–shell like particle morphologies are formed but without a sharp interface between calcium and strontium containing phases.
Surprisingly, the in-depth chemical distribution of the two types of nanoparticles is equal within the error of the experiment. Both comprise a SrF2-rich core domain and CaF2-rich shell domain with an intermixing zone between them. Consequently, the internal morphology of the final nanoparticles seems to be independent from the synthesis chronology.
Bis Mitte 2005 müssen schätzungsweise 250 alte Hausmülldeponien geschlossen werden, die nicht dem Stand der Technik entsprechen. Danach muß irgendwann eine Sicherung erfolgen. Wo dies im Einzelfall kontrollierbar möglich ist, kann man versuchen, den Deponiekörper anaerob ausreagieren zu lassen oder aerob zu stabilisieren. An einer zusätzlichen technischen Barriere wird jedoch auch dann kaum ein Weg vorbeiführen. Einfache, aber hochwirksame technische Abdichtungen können auch auf der Oberfläche einer Deponie errichtet werden. Für die dort wirksamen Beanspruchungen sind Abdichtungen mit ausgewählten PE-HD-Dichtungsbahnen besonders geeignet. Eine Zulassung der Produkte für diesen Anwendungszweck ist erforderlich, da PE-HD-Werkstoffe, aber auch Dichtungsbahnen, die aus dem gleichen PE-HD-Werkstoff unterschiedlich gefertigt wurden, sich in ihren Eigenschaften drastisch unterscheiden können.
Mit PE-HD-Dichtungsbahnen kann eine sehr wirksame, endgültige Oberflächenabdichtung auf einer Deponie gebaut werden. Dies setzt zwei Dinge voraus: die Dichtungsbahnen müssen fehlerfrei eingebaut werden und sie müssen lange genug halten. Die Lebensdauern von PE-HD-Dichtungsbahnen können sich jedoch je nach Werkstoff, Verarbeitung und Installation um Größenordnungen unterscheiden. Für die Auswahl sind daher spezielle Untersuchungen zur Alterung entscheidend und die Herstellungs-, Schweiß- und Verlegetechnik müssen bestimmte technische Standards erfüllen.
Durch die hydrolytische Alterung ändert sich die Zugfestigkeit eines Polyester-Bewehrungsgitters im Laufe der Zeit. Nach den Empfehlungen für den Entwurf und die Berechnung von Erdkörpern mit Bewehrung aus Geokunststoffen (EBGEO) der DGGT wird dieser Effekt durch einen Abminderungsfaktor bei der Bemessung berücksichtigt. Es ist zwar im Prinzip festgelegt, wie man bei der Bestimmung eines solchen Faktors für eine chemisch bedingte Materialveränderung vorgehen soll (ISO/TR 20432), es bleiben jedoch große Freiheiten bei der Umsetzung. Die Fragen, die sich daraus bei Bewehrungsgittern aus Polyester ergeben, werden diskutiert. Es werden Bausteine eines einheitlichen Verfahrens vorgeschlagen, das sich nicht nur auf den Festigkeitsverlust, sondern auch auf die molekulare Veränderung konzentriert.
Kunststoff-Dränelemente werden auch in Böschungen eingebaut. Da sie in der Regel aus mehreren Komponenten, nämlich mindestens aus einem Dränkern und einem Filtervliesstoff bestehen, hängt die Standsicherheit u. a. von der inneren Scherfestigkeit der Produkte ab. Diese kann entweder durch die reine Reibung der Komponenten untereinander oder durch die mechanische Festigkeit von Fügestellen zwischen den Komponenten bedingt sein, die schon bei der Produktion hergestellt werden. Im letzteren Fall ist nicht klar, wie Ergebnisse von Reibungsversuchen im Rahmenschergerät zu interpretieren sind. Vor diesem Hintergrund wird gezeigt, wie die Druck- und Scherkräfte, die ein Produkt langfristig aushalten kann, aus einem Reibungsversuch im Zusammenhang mit Kriechversuchen abgeleitet werden können. Dieses Vorgehen wird bei der Zulassung nach der Deponieverordnung für den Einsatz in Deponieabdichtungen angewendet.-----------------------------------------------------------------------------------------------------
Geocomposite drains (GCD) are used on long and steep slopes. Since they are usually composed of different components, at least a drain core in connection with a nonwoven filter geotextile, the internal shear strength is of significant relevance for the slope stability. The internal shear strength may be due to pure friction forces between the different components or due to the mechanical strength of the bonding between the components achieved in a special production process. In the latter case the interpretation of the results of friction shear box tests is quite unclear. Against this background it is shown how the pressure and shear forces, which are acceptable for a product in the long run, may be derived from such a shear box test in combination with long-term creep tests. The procedure is used within the framework of the certification of the products for landfill cover systems according to the German landfill ordinance.
Geogrids, which are installed to prevent sliding failure on long and steep slopes, have to be safely anchored. The design and calculation of the anchorage is based on simple design rules. Basically, it is assumed that the pull-out resistance is proportional to the soil shear strength, the vertical load and the anchoring length and that the soil-reinforcement coefficient of proportionality as determined in pull-out tests is typically in the range between 0.5 and 1. Based on an extended version of a model for the soil-geogrid interaction, which was described by Ziegler and Timmers (2004) and Sieira et al. (2009), the physical assumptions and limitations of these rules are discussed. For those geogrids, for which the passive thrust mobilization of earth pressure by the displacement of the transversal or bearing force grid elements substantially contributes to the pull-out resistance, the mechanical strength of the junction between longitudinal and transversal elements is of crucial importance. The relation between mechanical properties of the junction, the flexibility of the longitudinal grid elements, the surface friction and the finally achieved pull-out resistance is exemplarily shown by a model calculation. It is included, that due to aging and creep the short-term junction strength may be significantly lower than the long-term strength. There is a certain critical pull-out resistance and an associated critical anchorage length. Both are determined by the strength of the junction embedded into the soil and are independent from the actually installed anchorage length. For a safe design it is not allowed to go beyond that limit. This requirement restricts the range of application of the common design rules. It follows that not only the long-term strength of the longitudinal elements has to be considered and quantified by reduction factors but also the long-term strength of junctions. These limitations have to be observed to achieve a safe design of the anchorage. Preliminary design rules are discussed.